
data_global


data_c:\xray\mark\k08msh38\maxus\k08msh38
#TrackingRef '18979_web_deposit_cif_file_0_MSHill_1364469754.k08msh38.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H45 N2'
_chemical_formula_weight         541.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.1744(2)
_cell_length_b                   15.6545(4)
_cell_length_c                   16.8459(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.355(1)
_cell_angle_gamma                90.00
_cell_volume                     3257.32(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    41445
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1172
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55301
_diffrn_reflns_av_R_equivalents  0.1158
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.05
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6636
_reflns_number_gt                4150
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0742P)²+2.6321P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6636
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.1924
_refine_ls_wR_factor_gt          0.1621
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.54388(17) 0.20922(14) 0.21938(12) 0.0313(5) Uani 1 1 d . . .
N2 N 0.74761(16) 0.20347(14) 0.34695(13) 0.0306(5) Uani 1 1 d . . .
C1 C 0.5048(2) 0.20629(16) 0.27889(15) 0.0298(6) Uani 1 1 d . . .
C2 C 0.5782(2) 0.21186(17) 0.36466(15) 0.0319(6) Uani 1 1 d . . .
H2 H 0.5445 0.2155 0.4061 0.044(8) Uiso 1 1 calc R . .
C3 C 0.6957(2) 0.21288(16) 0.39839(15) 0.0297(6) Uani 1 1 d . . .
C4 C 0.7573(2) 0.22536(16) 0.49201(15) 0.0302(6) Uani 1 1 d . . .
C5 C 0.7185(2) 0.28778(18) 0.53023(17) 0.0361(6) Uani 1 1 d . . .
H5 H 0.6573 0.3210 0.4989 0.043 Uiso 1 1 calc R . .
C6 C 0.7714(2) 0.30155(19) 0.61720(17) 0.0419(7) Uani 1 1 d . . .
H6 H 0.7450 0.3451 0.6443 0.050 Uiso 1 1 calc R . .
C7 C 0.8632(2) 0.2529(2) 0.66670(17) 0.0428(7) Uani 1 1 d . . .
H7 H 0.8971 0.2644 0.7254 0.051 Uiso 1 1 calc R . .
C8 C 0.9015(2) 0.1905(2) 0.62934(17) 0.0405(7) Uani 1 1 d . . .
H8 H 0.9623 0.1572 0.6611 0.049 Uiso 1 1 calc R . .
C9 C 0.8491(2) 0.17606(18) 0.54254(16) 0.0348(6) Uani 1 1 d . . .
H9 H 0.8753 0.1319 0.5160 0.042 Uiso 1 1 calc R . .
C10 C 0.3828(2) 0.19586(17) 0.25706(15) 0.0301(6) Uani 1 1 d . . .
C11 C 0.3502(2) 0.13358(17) 0.29917(16) 0.0329(6) Uani 1 1 d . . .
H11 H 0.4020 0.0990 0.3399 0.040 Uiso 1 1 calc R . .
C12 C 0.2386(2) 0.12116(19) 0.28148(17) 0.0389(6) Uani 1 1 d . . .
H12 H 0.2164 0.0774 0.3110 0.047 Uiso 1 1 calc R . .
C13 C 0.1577(2) 0.1710(2) 0.22156(18) 0.0446(7) Uani 1 1 d . . .
H13 H 0.0832 0.1610 0.2115 0.053 Uiso 1 1 calc R . .
C14 C 0.1889(2) 0.2331(2) 0.17897(19) 0.0452(7) Uani 1 1 d . . .
H14 H 0.1369 0.2677 0.1385 0.054 Uiso 1 1 calc R . .
C15 C 0.3004(2) 0.24517(19) 0.19614(17) 0.0391(7) Uani 1 1 d . . .
H15 H 0.3221 0.2883 0.1657 0.047 Uiso 1 1 calc R . .
C16 C 0.47562(19) 0.20142(17) 0.13063(15) 0.0298(6) Uani 1 1 d . . .
C17 C 0.4585(2) 0.27511(18) 0.08040(17) 0.0370(6) Uani 1 1 d . . .
C18 C 0.3977(2) 0.2669(2) -0.00642(18) 0.0449(7) Uani 1 1 d . . .
H18 H 0.3859 0.3160 -0.0415 0.054 Uiso 1 1 calc R . .
C19 C 0.3542(2) 0.1891(2) -0.04253(18) 0.0504(8) Uani 1 1 d . . .
H19 H 0.3142 0.1854 -0.1014 0.060 Uiso 1 1 calc R . .
C20 C 0.3696(2) 0.1183(2) 0.00720(18) 0.0463(7) Uani 1 1 d . . .
H20 H 0.3380 0.0657 -0.0171 0.056 Uiso 1 1 calc R . .
C21 C 0.4321(2) 0.12193(18) 0.09488(16) 0.0357(6) Uani 1 1 d . . .
C22 C 0.4513(2) 0.04135(18) 0.14770(19) 0.0438(7) Uani 1 1 d . . .
H22 H 0.4821 0.0584 0.2086 0.066 Uiso 1 1 calc R . .
C23 C 0.3422(3) -0.0039(2) 0.1334(2) 0.0655(10) Uani 1 1 d . . .
H23A H 0.3546 -0.0558 0.1681 0.098 Uiso 1 1 calc R . .
H23B H 0.3088 -0.0192 0.0735 0.098 Uiso 1 1 calc R . .
H23C H 0.2939 0.0345 0.1495 0.098 Uiso 1 1 calc R . .
C24 C 0.5301(3) -0.0192(2) 0.1303(2) 0.0617(9) Uani 1 1 d . . .
H24A H 0.5398 -0.0696 0.1668 0.093 Uiso 1 1 calc R . .
H24B H 0.5999 0.0095 0.1421 0.093 Uiso 1 1 calc R . .
H24C H 0.5018 -0.0369 0.0708 0.093 Uiso 1 1 calc R . .
C25 C 0.5000(3) 0.3623(2) 0.1202(2) 0.0507(8) Uani 1 1 d . . .
H25 H 0.4953 0.3616 0.1782 0.076 Uiso 1 1 calc R . .
C26 C 0.6152(3) 0.3801(3) 0.1314(3) 0.0813(13) Uani 1 1 d . . .
H26A H 0.6355 0.4366 0.1572 0.122 Uiso 1 1 calc R . .
H26B H 0.6244 0.3791 0.0761 0.122 Uiso 1 1 calc R . .
H26C H 0.6617 0.3365 0.1682 0.122 Uiso 1 1 calc R . .
C27 C 0.4212(3) 0.4356(3) 0.0694(3) 0.0830(13) Uani 1 1 d . . .
H27A H 0.3465 0.4210 0.0633 0.125 Uiso 1 1 calc R . .
H27B H 0.4271 0.4416 0.0133 0.125 Uiso 1 1 calc R . .
H27C H 0.4413 0.4896 0.1004 0.125 Uiso 1 1 calc R . .
C28 C 0.8657(2) 0.19684(16) 0.37347(15) 0.0292(5) Uani 1 1 d . . .
C29 C 0.9373(2) 0.26679(17) 0.40614(15) 0.0325(6) Uani 1 1 d . . .
C30 C 1.0514(2) 0.2542(2) 0.42973(18) 0.0409(7) Uani 1 1 d . . .
H30 H 1.0991 0.3007 0.4523 0.049 Uiso 1 1 calc R . .
C31 C 1.0929(2) 0.1764(2) 0.42033(19) 0.0473(8) Uani 1 1 d . . .
H31 H 1.1690 0.1679 0.4378 0.057 Uiso 1 1 calc R . .
C32 C 1.0213(2) 0.1095(2) 0.3846(2) 0.0461(7) Uani 1 1 d . . .
H32 H 1.0504 0.0559 0.3768 0.055 Uiso 1 1 calc R . .
C33 C 0.9067(2) 0.11771(18) 0.35924(17) 0.0377(6) Uani 1 1 d . . .
C34 C 0.8296(3) 0.0428(2) 0.3193(2) 0.0547(8) Uani 1 1 d . . .
H34 H 0.7545 0.0657 0.2923 0.082 Uiso 1 1 calc R . .
C35 C 0.8588(3) -0.0066(2) 0.2557(2) 0.0616(9) Uani 1 1 d . . .
H35A H 0.8585 0.0312 0.2092 0.092 Uiso 1 1 calc R . .
H35B H 0.8061 -0.0526 0.2334 0.092 Uiso 1 1 calc R . .
H35C H 0.9312 -0.0312 0.2821 0.092 Uiso 1 1 calc R . .
C36 C 0.8306(6) -0.0182(3) 0.3875(3) 0.133(3) Uani 1 1 d . . .
H36A H 0.7816 -0.0659 0.3628 0.199 Uiso 1 1 calc R . .
H36B H 0.8066 0.0112 0.4292 0.199 Uiso 1 1 calc R . .
H36C H 0.9042 -0.0399 0.4153 0.199 Uiso 1 1 calc R . .
C37 C 0.8946(2) 0.35513(17) 0.41272(17) 0.0369(6) Uani 1 1 d . . .
H37 H 0.8149 0.3509 0.4007 0.055 Uiso 1 1 calc R . .
C38 C 0.9489(3) 0.3898(2) 0.50350(18) 0.0462(7) Uani 1 1 d . . .
H38A H 0.9208 0.4470 0.5075 0.069 Uiso 1 1 calc R . .
H38B H 1.0274 0.3928 0.5169 0.069 Uiso 1 1 calc R . .
H38C H 0.9329 0.3516 0.5437 0.069 Uiso 1 1 calc R . .
C39 C 0.9134(3) 0.4164(2) 0.35091(19) 0.0493(8) Uani 1 1 d . . .
H39A H 0.8842 0.4726 0.3572 0.074 Uiso 1 1 calc R . .
H39B H 0.8769 0.3955 0.2931 0.074 Uiso 1 1 calc R . .
H39C H 0.9912 0.4213 0.3619 0.074 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.277(3) . ?
N1 C16 1.457(3) . ?
N2 C3 1.285(3) . ?
N2 C28 1.465(3) . ?
C1 C2 1.435(3) . ?
C1 C10 1.527(3) . ?
C2 C3 1.452(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.515(3) . ?
C4 C5 1.364(4) . ?
C4 C9 1.438(4) . ?
C5 C6 1.403(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.426(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.352(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.401(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.360(4) . ?
C10 C15 1.433(4) . ?
C11 C12 1.409(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.419(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.354(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.407(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.402(4) . ?
C16 C21 1.414(4) . ?
C17 C18 1.408(4) . ?
C17 C25 1.534(4) . ?
C18 C19 1.392(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.360(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.420(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.513(4) . ?
C22 C24 1.508(4) . ?
C22 C23 1.545(4) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.490(5) . ?
C25 C27 1.585(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.405(4) . ?
C28 C29 1.425(4) . ?
C29 C30 1.429(4) . ?
C29 C37 1.511(4) . ?
C30 C31 1.368(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.399(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.424(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.545(4) . ?
C34 C35 1.478(4) . ?
C34 C36 1.489(6) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C39 1.498(4) . ?
C37 C38 1.544(4) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C16 121.9(2) . . ?
C3 N2 C28 124.0(2) . . ?
N1 C1 C2 118.3(2) . . ?
N1 C1 C10 119.5(2) . . ?
C2 C1 C10 122.2(2) . . ?
C1 C2 C3 130.4(2) . . ?
C1 C2 H2 114.8 . . ?
C3 C2 H2 114.8 . . ?
N2 C3 C2 118.7(2) . . ?
N2 C3 C4 119.9(2) . . ?
C2 C3 C4 121.4(2) . . ?
C5 C4 C9 118.8(2) . . ?
C5 C4 C3 115.5(2) . . ?
C9 C4 C3 125.7(2) . . ?
C4 C5 C6 118.1(3) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C5 C6 C7 122.7(3) . . ?
C5 C6 H6 118.6 . . ?
C7 C6 H6 118.6 . . ?
C8 C7 C6 119.4(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 118.3(3) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
C8 C9 C4 122.6(3) . . ?
C8 C9 H9 118.7 . . ?
C4 C9 H9 118.7 . . ?
C11 C10 C15 117.5(2) . . ?
C11 C10 C1 116.6(2) . . ?
C15 C10 C1 125.9(2) . . ?
C10 C11 C12 119.0(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C13 123.0(3) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 H12 118.5 . . ?
C14 C13 C12 118.7(3) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 118.3(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C10 123.5(3) . . ?
C14 C15 H15 118.3 . . ?
C10 C15 H15 118.3 . . ?
C17 C16 C21 120.7(2) . . ?
C17 C16 N1 117.6(2) . . ?
C21 C16 N1 121.6(2) . . ?
C16 C17 C18 117.7(3) . . ?
C16 C17 C25 120.7(2) . . ?
C18 C17 C25 121.5(3) . . ?
C19 C18 C17 122.2(3) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C20 C19 C18 119.5(3) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 121.1(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C20 118.7(3) . . ?
C16 C21 C22 121.5(2) . . ?
C20 C21 C22 119.8(3) . . ?
C24 C22 C21 113.3(2) . . ?
C24 C22 C23 110.3(3) . . ?
C21 C22 C23 109.6(3) . . ?
C24 C22 H22 107.8 . . ?
C21 C22 H22 107.8 . . ?
C23 C22 H22 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C17 114.5(3) . . ?
C26 C25 C27 112.3(3) . . ?
C17 C25 C27 110.0(3) . . ?
C26 C25 H25 106.5 . . ?
C17 C25 H25 106.5 . . ?
C27 C25 H25 106.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C33 C28 C29 120.1(2) . . ?
C33 C28 N2 116.2(2) . . ?
C29 C28 N2 123.6(2) . . ?
C28 C29 C30 119.5(2) . . ?
C28 C29 C37 121.2(2) . . ?
C30 C29 C37 119.2(2) . . ?
C31 C30 C29 121.0(3) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C32 118.7(3) . . ?
C30 C31 H31 120.7 . . ?
C32 C31 H31 120.7 . . ?
C31 C32 C33 123.2(3) . . ?
C31 C32 H32 118.4 . . ?
C33 C32 H32 118.4 . . ?
C28 C33 C32 117.3(3) . . ?
C28 C33 C34 120.6(2) . . ?
C32 C33 C34 122.0(3) . . ?
C35 C34 C36 106.8(3) . . ?
C35 C34 C33 114.5(3) . . ?
C36 C34 C33 108.8(3) . . ?
C35 C34 H34 108.8 . . ?
C36 C34 H34 108.8 . . ?
C33 C34 H34 108.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C39 C37 C29 112.3(2) . . ?
C39 C37 C38 109.4(2) . . ?
C29 C37 C38 109.8(2) . . ?
C39 C37 H37 108.4 . . ?
C29 C37 H37 108.4 . . ?
C38 C37 H37 108.4 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.049

data_global

# Attachment '18980_web_deposit_cif_file_1_MSHill_1364469754.k08msh54.cif'


data_c:\x-ray\kappa\k04360~1\maxus2\k08msh54
#TrackingRef '18980_web_deposit_cif_file_1_MSHill_1364469754.k08msh54.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H55 Li N2 O'
_chemical_formula_weight         622.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6640(3)
_cell_length_b                   12.0220(5)
_cell_length_c                   18.4070(9)
_cell_angle_alpha                86.906(2)
_cell_angle_beta                 83.488(2)
_cell_angle_gamma                81.211(2)
_cell_volume                     1881.20(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    102324
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   None
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26700
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.88
_diffrn_reflns_theta_max         27.00
_reflns_number_total             7817
_reflns_number_gt                5273
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0373P)²+1.1958P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0118(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7817
_refine_ls_number_parameters     425
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1452
_refine_ls_wR_factor_gt          0.1221
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7879(2) 0.02244(16) 0.80182(10) 0.0271(4) Uani 1 1 d . . .
C2 C 0.8099(2) 0.13374(16) 0.81284(11) 0.0284(4) Uani 1 1 d . . .
H2 H 0.8917 0.1414 0.8416 0.034 Uiso 1 1 calc R . .
C3 C 0.7262(2) 0.23596(16) 0.78664(10) 0.0274(4) Uani 1 1 d . . .
C4 C 0.8906(2) -0.06837(16) 0.84130(11) 0.0291(4) Uani 1 1 d . . .
C5 C 0.8993(2) -0.06429(18) 0.91591(11) 0.0345(5) Uani 1 1 d . . .
H5 H 0.8424 -0.0024 0.9421 0.041 Uiso 1 1 calc R . .
C6 C 0.9902(3) -0.14945(19) 0.95276(13) 0.0424(6) Uani 1 1 d . . .
H6 H 0.9937 -0.1465 1.0040 0.051 Uiso 1 1 calc R . .
C7 C 1.0756(3) -0.23853(19) 0.91446(14) 0.0470(6) Uani 1 1 d . . .
H7 H 1.1379 -0.2970 0.9394 0.056 Uiso 1 1 calc R . .
C8 C 1.0704(3) -0.24258(18) 0.84018(14) 0.0440(6) Uani 1 1 d . . .
H8 H 1.1310 -0.3031 0.8139 0.053 Uiso 1 1 calc R . .
C9 C 0.9773(2) -0.15886(16) 0.80370(12) 0.0356(5) Uani 1 1 d . . .
H9 H 0.9725 -0.1631 0.7526 0.043 Uiso 1 1 calc R . .
C10 C 0.7625(2) 0.34055(16) 0.81800(11) 0.0302(4) Uani 1 1 d . . .
C11 C 0.7588(3) 0.34711(18) 0.89331(12) 0.0397(5) Uani 1 1 d . . .
H11 H 0.7340 0.2851 0.9243 0.048 Uiso 1 1 calc R . .
C12 C 0.7906(3) 0.44269(19) 0.92390(13) 0.0478(6) Uani 1 1 d . . .
H12 H 0.7861 0.4462 0.9756 0.057 Uiso 1 1 calc R . .
C13 C 0.8287(3) 0.53272(18) 0.87976(14) 0.0452(6) Uani 1 1 d . . .
H13 H 0.8503 0.5983 0.9008 0.054 Uiso 1 1 calc R . .
C14 C 0.8354(3) 0.52730(17) 0.80489(13) 0.0400(5) Uani 1 1 d . . .
H14 H 0.8633 0.5888 0.7742 0.048 Uiso 1 1 calc R . .
C15 C 0.8017(2) 0.43218(16) 0.77428(12) 0.0337(5) Uani 1 1 d . . .
H15 H 0.8053 0.4295 0.7226 0.040 Uiso 1 1 calc R . .
C16 C 0.5244(2) 0.34002(16) 0.71755(11) 0.0293(4) Uani 1 1 d . . .
C17 C 0.3865(2) 0.38129(16) 0.76256(12) 0.0325(5) Uani 1 1 d . . .
C18 C 0.2766(3) 0.46362(17) 0.73294(12) 0.0377(5) Uani 1 1 d . . .
H18 H 0.1822 0.4906 0.7622 0.045 Uiso 1 1 calc R . .
C19 C 0.3013(3) 0.50659(18) 0.66270(13) 0.0414(5) Uani 1 1 d . . .
H19 H 0.2240 0.5614 0.6435 0.050 Uiso 1 1 calc R . .
C20 C 0.4397(3) 0.46935(18) 0.62016(12) 0.0395(5) Uani 1 1 d . . .
H20 H 0.4584 0.5014 0.5722 0.047 Uiso 1 1 calc R . .
C21 C 0.5522(2) 0.38605(17) 0.64596(11) 0.0325(5) Uani 1 1 d . . .
C22 C 0.3538(3) 0.33908(18) 0.84091(12) 0.0390(5) Uani 1 1 d . . .
H22 H 0.4435 0.2800 0.8520 0.047 Uiso 1 1 calc R . .
C23 C 0.2030(3) 0.2851(2) 0.85292(16) 0.0595(7) Uani 1 1 d . . .
H23A H 0.1862 0.2588 0.9041 0.089 Uiso 1 1 calc R . .
H23B H 0.2129 0.2212 0.8210 0.089 Uiso 1 1 calc R . .
H23C H 0.1135 0.3410 0.8413 0.089 Uiso 1 1 calc R . .
C24 C 0.3456(4) 0.4344(2) 0.89346(13) 0.0597(7) Uani 1 1 d . . .
H24A H 0.3248 0.4057 0.9439 0.090 Uiso 1 1 calc R . .
H24B H 0.2610 0.4948 0.8825 0.090 Uiso 1 1 calc R . .
H24C H 0.4459 0.4639 0.8877 0.090 Uiso 1 1 calc R . .
C25 C 0.6988(3) 0.34242(19) 0.59621(12) 0.0393(5) Uani 1 1 d . . .
H25 H 0.7729 0.2948 0.6272 0.047 Uiso 1 1 calc R . .
C26 C 0.6599(3) 0.2677(2) 0.53829(14) 0.0558(7) Uani 1 1 d . . .
H26A H 0.7561 0.2401 0.5071 0.084 Uiso 1 1 calc R . .
H26B H 0.5840 0.3114 0.5082 0.084 Uiso 1 1 calc R . .
H26C H 0.6147 0.2035 0.5624 0.084 Uiso 1 1 calc R . .
C27 C 0.7838(3) 0.4373(2) 0.55952(13) 0.0486(6) Uani 1 1 d . . .
H27A H 0.8774 0.4047 0.5285 0.073 Uiso 1 1 calc R . .
H27B H 0.8150 0.4814 0.5972 0.073 Uiso 1 1 calc R . .
H27C H 0.7131 0.4865 0.5295 0.073 Uiso 1 1 calc R . .
C28 C 0.6442(2) -0.11412(16) 0.76013(11) 0.0295(4) Uani 1 1 d . . .
C29 C 0.5539(2) -0.15775(16) 0.82087(11) 0.0318(5) Uani 1 1 d . . .
C30 C 0.4955(3) -0.25791(17) 0.81340(13) 0.0379(5) Uani 1 1 d . . .
H30 H 0.4358 -0.2886 0.8540 0.045 Uiso 1 1 calc R . .
C31 C 0.5221(3) -0.31339(18) 0.74863(13) 0.0412(5) Uani 1 1 d . . .
H31 H 0.4786 -0.3804 0.7445 0.049 Uiso 1 1 calc R . .
C32 C 0.6121(3) -0.27153(18) 0.68964(13) 0.0403(5) Uani 1 1 d . . .
H32 H 0.6305 -0.3104 0.6452 0.048 Uiso 1 1 calc R . .
C33 C 0.6762(2) -0.17306(17) 0.69452(11) 0.0340(5) Uani 1 1 d . . .
C34 C 0.5091(3) -0.09315(18) 0.89097(11) 0.0354(5) Uani 1 1 d . . .
H34 H 0.5926 -0.0456 0.8949 0.042 Uiso 1 1 calc R . .
C35 C 0.3549(3) -0.0138(2) 0.88661(13) 0.0474(6) Uani 1 1 d . . .
H35A H 0.3277 0.0271 0.9320 0.071 Uiso 1 1 calc R . .
H35B H 0.2713 -0.0576 0.8798 0.071 Uiso 1 1 calc R . .
H35C H 0.3666 0.0400 0.8452 0.071 Uiso 1 1 calc R . .
C36 C 0.5007(3) -0.1695(2) 0.95972(13) 0.0546(7) Uani 1 1 d . . .
H36A H 0.4718 -0.1233 1.0028 0.082 Uiso 1 1 calc R . .
H36B H 0.6034 -0.2154 0.9635 0.082 Uiso 1 1 calc R . .
H36C H 0.4216 -0.2189 0.9570 0.082 Uiso 1 1 calc R . .
C37 C 0.7773(3) -0.12917(19) 0.63003(12) 0.0426(6) Uani 1 1 d . . .
H37 H 0.8360 -0.0733 0.6489 0.051 Uiso 1 1 calc R . .
C38 C 0.6781(4) -0.0677(2) 0.57275(14) 0.0619(7) Uani 1 1 d . . .
H38A H 0.7471 -0.0402 0.5320 0.093 Uiso 1 1 calc R . .
H38B H 0.6078 -0.0038 0.5948 0.093 Uiso 1 1 calc R . .
H38C H 0.6157 -0.1195 0.5545 0.093 Uiso 1 1 calc R . .
C39 C 0.8995(3) -0.2218(2) 0.59396(16) 0.0615(7) Uani 1 1 d . . .
H39A H 0.9617 -0.1887 0.5529 0.092 Uiso 1 1 calc R . .
H39B H 0.8457 -0.2792 0.5760 0.092 Uiso 1 1 calc R . .
H39C H 0.9690 -0.2565 0.6300 0.092 Uiso 1 1 calc R . .
C40 C 0.2665(3) 0.1807(2) 0.63201(14) 0.0488(6) Uani 1 1 d . . .
H40A H 0.2726 0.1491 0.5830 0.059 Uiso 1 1 calc R . .
H40B H 0.3262 0.2451 0.6270 0.059 Uiso 1 1 calc R . .
C41 C 0.0993(3) 0.2232(3) 0.65625(19) 0.0723(9) Uani 1 1 d . . .
H41A H 0.0579 0.2804 0.6206 0.108 Uiso 1 1 calc R . .
H41B H 0.0917 0.2566 0.7042 0.108 Uiso 1 1 calc R . .
H41C H 0.0380 0.1606 0.6600 0.108 Uiso 1 1 calc R . .
C42 C 0.2619(3) -0.0015(2) 0.69727(13) 0.0468(6) Uani 1 1 d . . .
H42A H 0.1588 0.0232 0.7251 0.056 Uiso 1 1 calc R . .
H42B H 0.3245 -0.0550 0.7293 0.056 Uiso 1 1 calc R . .
C43 C 0.2358(4) -0.0623(2) 0.63144(15) 0.0620(7) Uani 1 1 d . . .
H43A H 0.1820 -0.1269 0.6474 0.093 Uiso 1 1 calc R . .
H43B H 0.3373 -0.0889 0.6040 0.093 Uiso 1 1 calc R . .
H43C H 0.1711 -0.0109 0.6000 0.093 Uiso 1 1 calc R . .
N1 N 0.62234(19) 0.23979(13) 0.73867(9) 0.0288(4) Uani 1 1 d . . .
N2 N 0.68425(19) -0.00360(13) 0.76013(9) 0.0294(4) Uani 1 1 d . . .
O1 O 0.34152(17) 0.09575(12) 0.68018(8) 0.0407(4) Uani 1 1 d . . .
Li1 Li 0.5404(4) 0.1083(3) 0.7142(2) 0.0377(8) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.327(2) . ?
C1 C2 1.409(3) . ?
C1 C4 1.509(3) . ?
C2 C3 1.418(3) . ?
C3 N1 1.324(2) . ?
C3 C10 1.501(3) . ?
C4 C5 1.388(3) . ?
C4 C9 1.393(3) . ?
C5 C6 1.388(3) . ?
C6 C7 1.383(3) . ?
C7 C8 1.377(3) . ?
C8 C9 1.384(3) . ?
C10 C11 1.389(3) . ?
C10 C15 1.390(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.376(3) . ?
C13 C14 1.377(3) . ?
C14 C15 1.386(3) . ?
C16 C21 1.411(3) . ?
C16 C17 1.414(3) . ?
C16 N1 1.426(2) . ?
C16 Li1 2.772(4) . ?
C17 C18 1.398(3) . ?
C17 C22 1.513(3) . ?
C18 C19 1.372(3) . ?
C19 C20 1.383(3) . ?
C20 C21 1.391(3) . ?
C21 C25 1.520(3) . ?
C22 C24 1.528(3) . ?
C22 C23 1.535(3) . ?
C25 C26 1.528(3) . ?
C25 C27 1.537(3) . ?
C28 C33 1.412(3) . ?
C28 C29 1.415(3) . ?
C28 N2 1.424(2) . ?
C29 C30 1.395(3) . ?
C29 C34 1.523(3) . ?
C30 C31 1.377(3) . ?
C31 C32 1.382(3) . ?
C32 C33 1.393(3) . ?
C33 C37 1.514(3) . ?
C34 C36 1.524(3) . ?
C34 C35 1.526(3) . ?
C37 C38 1.525(3) . ?
C37 C39 1.536(3) . ?
C40 O1 1.442(3) . ?
C40 C41 1.487(4) . ?
C42 O1 1.449(3) . ?
C42 C43 1.504(3) . ?
N1 Li1 1.924(4) . ?
N2 Li1 1.919(4) . ?
O1 Li1 1.928(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 123.61(17) . . ?
N2 C1 C4 120.83(17) . . ?
C2 C1 C4 115.56(17) . . ?
C1 C2 C3 128.61(18) . . ?
N1 C3 C2 123.00(18) . . ?
N1 C3 C10 122.03(17) . . ?
C2 C3 C10 114.96(17) . . ?
C5 C4 C9 118.58(19) . . ?
C5 C4 C1 120.80(18) . . ?
C9 C4 C1 120.62(18) . . ?
C4 C5 C6 120.9(2) . . ?
C7 C6 C5 119.6(2) . . ?
C8 C7 C6 120.1(2) . . ?
C7 C8 C9 120.2(2) . . ?
C8 C9 C4 120.5(2) . . ?
C11 C10 C15 117.97(19) . . ?
C11 C10 C3 119.62(18) . . ?
C15 C10 C3 122.41(18) . . ?
C12 C11 C10 121.0(2) . . ?
C13 C12 C11 120.2(2) . . ?
C12 C13 C14 119.7(2) . . ?
C13 C14 C15 120.0(2) . . ?
C14 C15 C10 121.0(2) . . ?
C21 C16 C17 119.99(18) . . ?
C21 C16 N1 118.69(18) . . ?
C17 C16 N1 120.44(17) . . ?
C21 C16 Li1 110.08(15) . . ?
C17 C16 Li1 107.61(15) . . ?
N1 C16 Li1 40.44(11) . . ?
C18 C17 C16 118.33(19) . . ?
C18 C17 C22 119.27(19) . . ?
C16 C17 C22 122.40(18) . . ?
C19 C18 C17 121.8(2) . . ?
C18 C19 C20 119.4(2) . . ?
C19 C20 C21 121.5(2) . . ?
C20 C21 C16 118.9(2) . . ?
C20 C21 C25 120.06(19) . . ?
C16 C21 C25 121.03(18) . . ?
C17 C22 C24 110.50(18) . . ?
C17 C22 C23 112.0(2) . . ?
C24 C22 C23 110.6(2) . . ?
C21 C25 C26 110.88(19) . . ?
C21 C25 C27 112.83(19) . . ?
C26 C25 C27 110.17(19) . . ?
C33 C28 C29 120.02(18) . . ?
C33 C28 N2 118.55(18) . . ?
C29 C28 N2 120.79(17) . . ?
C30 C29 C28 118.37(19) . . ?
C30 C29 C34 119.99(19) . . ?
C28 C29 C34 121.45(17) . . ?
C31 C30 C29 121.6(2) . . ?
C30 C31 C32 120.0(2) . . ?
C31 C32 C33 120.9(2) . . ?
C32 C33 C28 119.1(2) . . ?
C32 C33 C37 120.44(19) . . ?
C28 C33 C37 120.44(18) . . ?
C29 C34 C36 113.26(18) . . ?
C29 C34 C35 110.46(17) . . ?
C36 C34 C35 110.8(2) . . ?
C33 C37 C38 111.6(2) . . ?
C33 C37 C39 113.0(2) . . ?
C38 C37 C39 109.8(2) . . ?
O1 C40 C41 114.9(2) . . ?
O1 C42 C43 114.3(2) . . ?
C3 N1 C16 124.01(17) . . ?
C3 N1 Li1 122.48(17) . . ?
C16 N1 Li1 110.81(16) . . ?
C1 N2 C28 122.38(16) . . ?
C1 N2 Li1 122.69(17) . . ?
C28 N2 Li1 113.26(16) . . ?
C40 O1 C42 115.40(17) . . ?
C40 O1 Li1 121.63(17) . . ?
C42 O1 Li1 122.86(17) . . ?
N2 Li1 N1 98.31(17) . . ?
N2 Li1 O1 129.7(2) . . ?
N1 Li1 O1 129.8(2) . . ?
N2 Li1 C16 126.84(17) . . ?
N1 Li1 C16 28.75(8) . . ?
O1 Li1 C16 101.30(15) . . ?

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.045

data_global

# Attachment '18981_web_deposit_cif_file_2_MSHill_1364469754.h12msh2.cif'


data_h12msh2
#TrackingRef '18981_web_deposit_cif_file_2_MSHill_1364469754.h12msh2.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H53 Be I N2 O'
_chemical_formula_sum            'C43 H53 Be I N2 O'
_chemical_formula_weight         749.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4935(2)
_cell_length_b                   12.0951(2)
_cell_length_c                   19.6152(3)
_cell_angle_alpha                97.7550(12)
_cell_angle_beta                 97.8470(12)
_cell_angle_gamma                102.2030(11)
_cell_volume                     1922.97(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    40861
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7810
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '361 1.7 degree images with φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            39575
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.11
_diffrn_reflns_theta_max         27.49
_reflns_number_total             8746
_reflns_number_gt                7205
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
;
DENZO-SCALEPACK Z. Otwinowski and W. Minor, "
Processing of X-ray Diffraction Data Collected in Oscillation Mode ",
Methods in Enzymology, Volume 276: Macromolecular Crystallography,
part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_structure_solution    
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119
;
_computing_structure_refinement  
;
Sheldrick GM (2008) Acta Crystallogr A64:112--122 and
C. B. Hübschle, G. M. Sheldrick and B. Dittrich
ShelXle: a Qt graphical user interface for SHELXL
J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
'WinGX publication routines, Farrugia,
L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0499P)²+3.7415P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8746
_refine_ls_number_parameters     460
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1180
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Be Be 0.7655(4) 0.0024(3) 0.22865(18) 0.0236(7) Uani 1 1 d . . .
I I 0.75592(3) -0.43363(2) 0.010619(14) 0.05303(10) Uani 1 1 d . . .
N1 N 0.7070(3) -0.08717(18) 0.28147(11) 0.0222(4) Uani 1 1 d . . .
N2 N 0.7568(3) 0.13256(18) 0.26173(11) 0.0204(4) Uani 1 1 d . . .
C1 C 0.6742(3) -0.0480(2) 0.34370(14) 0.0233(5) Uani 1 1 d . . .
C2 C 0.6392(3) -0.1241(2) 0.39678(14) 0.0253(5) Uani 1 1 d . . .
C3 C 0.5176(4) -0.2248(2) 0.38213(15) 0.0282(6) Uani 1 1 d . . .
H3 H 0.4574 -0.2500 0.3361 0.034 Uiso 1 1 calc R . .
C4 C 0.4832(4) -0.2891(3) 0.43424(16) 0.0325(6) Uani 1 1 d . . .
H4 H 0.3992 -0.3577 0.4237 0.039 Uiso 1 1 calc R . .
C5 C 0.5707(4) -0.2536(3) 0.50144(17) 0.0361(7) Uani 1 1 d . . .
H5 H 0.5458 -0.2970 0.5371 0.043 Uiso 1 1 calc R . .
C6 C 0.6944(5) -0.1547(3) 0.51632(17) 0.0414(8) Uani 1 1 d . . .
H6 H 0.7565 -0.1310 0.5621 0.050 Uiso 1 1 calc R . .
C7 C 0.7281(4) -0.0901(3) 0.46446(16) 0.0370(7) Uani 1 1 d . . .
H7 H 0.8127 -0.0219 0.4751 0.044 Uiso 1 1 calc R . .
C8 C 0.6750(3) 0.0676(2) 0.36401(14) 0.0246(5) Uani 1 1 d . . .
H8 H 0.6425 0.0882 0.4075 0.030 Uiso 1 1 calc R . .
C9 C 0.7199(3) 0.1560(2) 0.32550(13) 0.0214(5) Uani 1 1 d . . .
C10 C 0.7290(3) 0.2746(2) 0.36094(13) 0.0222(5) Uani 1 1 d . . .
C11 C 0.8054(3) 0.3081(2) 0.43079(14) 0.0261(5) Uani 1 1 d . . .
H11 H 0.8538 0.2562 0.4538 0.031 Uiso 1 1 calc R . .
C12 C 0.8115(4) 0.4160(2) 0.46684(15) 0.0305(6) Uani 1 1 d . . .
H12 H 0.8640 0.4377 0.5142 0.037 Uiso 1 1 calc R . .
C13 C 0.7407(4) 0.4926(2) 0.43378(16) 0.0332(6) Uani 1 1 d . . .
H13 H 0.7446 0.5666 0.4585 0.040 Uiso 1 1 calc R . .
C14 C 0.6646(4) 0.4607(2) 0.36489(16) 0.0323(6) Uani 1 1 d . . .
H14 H 0.6153 0.5128 0.3424 0.039 Uiso 1 1 calc R . .
C15 C 0.6596(3) 0.3528(2) 0.32832(14) 0.0265(5) Uani 1 1 d . . .
H15 H 0.6084 0.3321 0.2807 0.032 Uiso 1 1 calc R . .
C16 C 0.7223(3) -0.2045(2) 0.26415(13) 0.0237(5) Uani 1 1 d . . .
C17 C 0.5981(4) -0.2833(2) 0.21613(15) 0.0278(6) Uani 1 1 d . . .
C18 C 0.4410(4) -0.2532(3) 0.18596(16) 0.0331(6) Uani 1 1 d . . .
H18 H 0.4329 -0.1803 0.2145 0.040 Uiso 1 1 calc R . .
C19 C 0.4434(4) -0.2336(3) 0.11007(19) 0.0439(8) Uani 1 1 d . . .
H19A H 0.4518 -0.3043 0.0812 0.066 Uiso 1 1 calc R . .
H19B H 0.5376 -0.1716 0.1088 0.066 Uiso 1 1 calc R . .
H19C H 0.3424 -0.2126 0.0919 0.066 Uiso 1 1 calc R . .
C20 C 0.2891(4) -0.3470(3) 0.18846(19) 0.0439(8) Uani 1 1 d . . .
H20A H 0.1905 -0.3187 0.1769 0.066 Uiso 1 1 calc R . .
H20B H 0.2949 -0.3667 0.2355 0.066 Uiso 1 1 calc R . .
H20C H 0.2851 -0.4154 0.1546 0.066 Uiso 1 1 calc R . .
C21 C 0.6222(4) -0.3925(2) 0.19505(16) 0.0345(7) Uani 1 1 d . . .
H21 H 0.5395 -0.4470 0.1626 0.041 Uiso 1 1 calc R . .
C22 C 0.7641(4) -0.4229(3) 0.22048(17) 0.0382(7) Uani 1 1 d . . .
H22 H 0.7787 -0.4975 0.2054 0.046 Uiso 1 1 calc R . .
C23 C 0.8845(4) -0.3445(3) 0.26789(16) 0.0345(7) Uani 1 1 d . . .
H23 H 0.9813 -0.3662 0.2854 0.041 Uiso 1 1 calc R . .
C24 C 0.8673(4) -0.2336(2) 0.29086(14) 0.0274(6) Uani 1 1 d . . .
C25 C 1.0077(4) -0.1490(3) 0.34039(16) 0.0334(6) Uani 1 1 d . . .
H25 H 0.9678 -0.0800 0.3575 0.040 Uiso 1 1 calc R . .
C26 C 1.0670(5) -0.2000(3) 0.40408(19) 0.0492(9) Uani 1 1 d . . .
H26A H 1.1061 -0.2682 0.3884 0.074 Uiso 1 1 calc R . .
H26B H 0.9764 -0.2214 0.4294 0.074 Uiso 1 1 calc R . .
H26C H 1.1563 -0.1429 0.4350 0.074 Uiso 1 1 calc R . .
C27 C 1.1491(4) -0.1105(3) 0.3017(2) 0.0446(8) Uani 1 1 d . . .
H27A H 1.1914 -0.1768 0.2852 0.067 Uiso 1 1 calc R . .
H27B H 1.2365 -0.0530 0.3334 0.067 Uiso 1 1 calc R . .
H27C H 1.1100 -0.0771 0.2617 0.067 Uiso 1 1 calc R . .
C28 C 0.8192(3) 0.2215(2) 0.22334(13) 0.0212(5) Uani 1 1 d . . .
C29 C 0.9833(3) 0.2830(2) 0.24160(14) 0.0247(5) Uani 1 1 d . . .
C30 C 1.0949(3) 0.2721(3) 0.30643(15) 0.0296(6) Uani 1 1 d . . .
H30 H 1.0266 0.2250 0.3346 0.036 Uiso 1 1 calc R . .
C31 C 1.2245(4) 0.2090(3) 0.28667(18) 0.0403(7) Uani 1 1 d . . .
H31A H 1.1709 0.1333 0.2592 0.060 Uiso 1 1 calc R . .
H31B H 1.2924 0.1999 0.3292 0.060 Uiso 1 1 calc R . .
H31C H 1.2934 0.2535 0.2589 0.060 Uiso 1 1 calc R . .
C32 C 1.1728(5) 0.3893(3) 0.35152(19) 0.0463(8) Uani 1 1 d . . .
H32A H 1.2478 0.4350 0.3266 0.069 Uiso 1 1 calc R . .
H32B H 1.2334 0.3790 0.3955 0.069 Uiso 1 1 calc R . .
H32C H 1.0871 0.4291 0.3614 0.069 Uiso 1 1 calc R . .
C33 C 1.0468(4) 0.3544(2) 0.19632(16) 0.0307(6) Uani 1 1 d . . .
H33 H 1.1574 0.3966 0.2077 0.037 Uiso 1 1 calc R . .
C34 C 0.9518(4) 0.3645(2) 0.13560(16) 0.0321(6) Uani 1 1 d . . .
H34 H 0.9978 0.4118 0.1050 0.039 Uiso 1 1 calc R . .
C35 C 0.7896(4) 0.3059(2) 0.11942(15) 0.0297(6) Uani 1 1 d . . .
H35 H 0.7247 0.3140 0.0778 0.036 Uiso 1 1 calc R . .
C36 C 0.7189(3) 0.2347(2) 0.16306(13) 0.0234(5) Uani 1 1 d . . .
C37 C 0.5380(4) 0.1754(2) 0.14461(15) 0.0290(6) Uani 1 1 d . . .
H37 H 0.5052 0.1404 0.1854 0.035 Uiso 1 1 calc R . .
C38 C 0.4323(4) 0.2607(3) 0.12989(17) 0.0371(7) Uani 1 1 d . . .
H38A H 0.4536 0.2894 0.0869 0.056 Uiso 1 1 calc R . .
H38B H 0.4592 0.3250 0.1689 0.056 Uiso 1 1 calc R . .
H38C H 0.3165 0.2220 0.1245 0.056 Uiso 1 1 calc R . .
C39 C 0.5052(4) 0.0797(3) 0.08187(19) 0.0448(8) Uani 1 1 d . . .
H39A H 0.3888 0.0412 0.0723 0.067 Uiso 1 1 calc R . .
H39B H 0.5702 0.0241 0.0919 0.067 Uiso 1 1 calc R . .
H39C H 0.5353 0.1123 0.0411 0.067 Uiso 1 1 calc R . .
O O 0.8303(3) -0.03822(17) 0.16662(11) 0.0341(5) Uani 1 1 d . . .
C40 C 0.9146(4) 0.0062(3) 0.11698(17) 0.0377(7) Uani 1 1 d . A .
H40A H 0.9852 0.0826 0.1382 0.045 Uiso 1 1 calc R . .
H40B H 0.8349 0.0170 0.0781 0.045 Uiso 1 1 calc R . .
C41 C 1.0178(5) -0.0680(4) 0.0884(2) 0.0551(10) Uani 1 1 d D . .
H41A H 1.0937 -0.0218 0.0632 0.066 Uiso 0.570(11) 1 calc PR A 1
H41B H 1.0851 -0.0874 0.1283 0.066 Uiso 0.570(11) 1 calc PR A 1
H41C H 1.1191 -0.0596 0.1221 0.066 Uiso 0.430(11) 1 calc PR A 2
H41D H 1.0482 -0.0460 0.0443 0.066 Uiso 0.430(11) 1 calc PR A 2
C42 C 0.9350(11) -0.1753(6) 0.0412(4) 0.051(2) Uani 0.570(11) 1 d P A 1
H42A H 0.8410 -0.1627 0.0099 0.062 Uiso 0.570(11) 1 calc PR A 1
H42B H 1.0115 -0.2000 0.0119 0.062 Uiso 0.570(11) 1 calc PR A 1
C43 C 0.8776(9) -0.2647(6) 0.0812(3) 0.047(2) Uani 0.570(11) 1 d P A 1
H43A H 0.7989 -0.2405 0.1094 0.057 Uiso 0.570(11) 1 calc PR A 1
H43B H 0.9715 -0.2751 0.1136 0.057 Uiso 0.570(11) 1 calc PR A 1
C42A C 0.913(3) -0.1962(9) 0.0748(10) 0.166(13) Uani 0.430(11) 1 d PD A 2
H42C H 0.9045 -0.2161 0.1217 0.199 Uiso 0.430(11) 1 calc PR A 2
H42D H 0.8016 -0.1927 0.0538 0.199 Uiso 0.430(11) 1 calc PR A 2
C43A C 0.9458(14) -0.2958(9) 0.0344(6) 0.075(4) Uani 0.430(11) 1 d PD A 2
H43C H 1.0393 -0.3171 0.0610 0.090 Uiso 0.430(11) 1 calc PR A 2
H43D H 0.9786 -0.2747 -0.0095 0.090 Uiso 0.430(11) 1 calc PR A 2


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Be O 1.470(4) . ?
Be N2 1.641(4) . ?
Be N1 1.646(4) . ?
I C43A 2.011(10) . ?
I C43 2.261(6) . ?
N1 C1 1.335(3) . ?
N1 C16 1.452(3) . ?
N2 C9 1.339(3) . ?
N2 C28 1.446(3) . ?
C1 C8 1.399(4) . ?
C1 C2 1.499(3) . ?
C2 C3 1.387(4) . ?
C2 C7 1.396(4) . ?
C3 C4 1.391(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.409(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.489(4) . ?
C10 C15 1.395(4) . ?
C10 C11 1.400(4) . ?
C11 C12 1.385(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.390(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.392(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.404(4) . ?
C16 C24 1.404(4) . ?
C17 C21 1.396(4) . ?
C17 C18 1.520(4) . ?
C18 C20 1.539(4) . ?
C18 C19 1.541(5) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.382(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.399(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.521(4) . ?
C25 C27 1.531(5) . ?
C25 C26 1.537(4) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.407(4) . ?
C28 C36 1.408(4) . ?
C29 C33 1.402(4) . ?
C29 C30 1.517(4) . ?
C30 C31 1.528(4) . ?
C30 C32 1.528(4) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.380(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.398(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.523(4) . ?
C37 C39 1.522(4) . ?
C37 C38 1.535(4) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
O C40 1.385(4) . ?
C40 C41 1.490(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.465(8) . ?
C41 C42A 1.584(12) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 H41C 0.9900 . ?
C41 H41D 0.9900 . ?
C42 C43 1.460(11) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C42A C43A 1.449(13) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Be N2 130.1(2) . . ?
O Be N1 119.7(2) . . ?
N2 Be N1 109.9(2) . . ?
C1 N1 C16 121.0(2) . . ?
C1 N1 Be 120.3(2) . . ?
C16 N1 Be 117.6(2) . . ?
C9 N2 C28 122.5(2) . . ?
C9 N2 Be 121.3(2) . . ?
C28 N2 Be 115.4(2) . . ?
N1 C1 C8 121.9(2) . . ?
N1 C1 C2 122.2(2) . . ?
C8 C1 C2 115.9(2) . . ?
C3 C2 C7 118.6(2) . . ?
C3 C2 C1 122.6(2) . . ?
C7 C2 C1 118.7(2) . . ?
C2 C3 C4 120.5(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 120.8(3) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C1 C8 C9 125.6(2) . . ?
C1 C8 H8 117.2 . . ?
C9 C8 H8 117.2 . . ?
N2 C9 C8 120.7(2) . . ?
N2 C9 C10 123.2(2) . . ?
C8 C9 C10 116.1(2) . . ?
C15 C10 C11 118.4(2) . . ?
C15 C10 C9 122.8(2) . . ?
C11 C10 C9 118.7(2) . . ?
C12 C11 C10 120.9(3) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.0(3) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 120.4(3) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C10 120.5(3) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
C17 C16 C24 121.6(2) . . ?
C17 C16 N1 119.0(2) . . ?
C24 C16 N1 119.2(2) . . ?
C21 C17 C16 118.1(3) . . ?
C21 C17 C18 119.4(3) . . ?
C16 C17 C18 122.5(2) . . ?
C17 C18 C20 111.9(3) . . ?
C17 C18 C19 110.7(3) . . ?
C20 C18 C19 109.5(3) . . ?
C17 C18 H18 108.2 . . ?
C20 C18 H18 108.2 . . ?
C19 C18 H18 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C17 121.3(3) . . ?
C22 C21 H21 119.3 . . ?
C17 C21 H21 119.3 . . ?
C23 C22 C21 119.7(3) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 121.6(3) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C23 C24 C16 117.7(3) . . ?
C23 C24 C25 119.2(3) . . ?
C16 C24 C25 123.0(2) . . ?
C24 C25 C27 110.1(3) . . ?
C24 C25 C26 111.8(3) . . ?
C27 C25 C26 110.4(3) . . ?
C24 C25 H25 108.1 . . ?
C27 C25 H25 108.1 . . ?
C26 C25 H25 108.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C36 121.2(2) . . ?
C29 C28 N2 119.8(2) . . ?
C36 C28 N2 118.5(2) . . ?
C33 C29 C28 118.0(2) . . ?
C33 C29 C30 119.0(2) . . ?
C28 C29 C30 122.9(2) . . ?
C29 C30 C31 110.7(2) . . ?
C29 C30 C32 111.3(3) . . ?
C31 C30 C32 111.4(3) . . ?
C29 C30 H30 107.8 . . ?
C31 C30 H30 107.8 . . ?
C32 C30 H30 107.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C29 121.3(3) . . ?
C34 C33 H33 119.4 . . ?
C29 C33 H33 119.4 . . ?
C33 C34 C35 119.9(3) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C36 121.4(3) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C36 C28 118.1(2) . . ?
C35 C36 C37 119.6(2) . . ?
C28 C36 C37 122.3(2) . . ?
C39 C37 C36 111.2(3) . . ?
C39 C37 C38 109.6(3) . . ?
C36 C37 C38 111.6(2) . . ?
C39 C37 H37 108.1 . . ?
C36 C37 H37 108.1 . . ?
C38 C37 H37 108.1 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C40 O Be 139.3(2) . . ?
O C40 C41 113.5(3) . . ?
O C40 H40A 108.9 . . ?
C41 C40 H40A 108.9 . . ?
O C40 H40B 108.9 . . ?
C41 C40 H40B 108.9 . . ?
H40A C40 H40B 107.7 . . ?
C42 C41 C40 117.9(5) . . ?
C40 C41 C42A 107.1(7) . . ?
C42 C41 H41A 107.8 . . ?
C40 C41 H41A 107.8 . . ?
C42A C41 H41A 135.1 . . ?
C42 C41 H41B 107.8 . . ?
C40 C41 H41B 107.8 . . ?
C42A C41 H41B 87.8 . . ?
H41A C41 H41B 107.2 . . ?
C42 C41 H41C 123.3 . . ?
C40 C41 H41C 110.3 . . ?
C42A C41 H41C 110.3 . . ?
C42 C41 H41D 81.5 . . ?
C40 C41 H41D 110.3 . . ?
C42A C41 H41D 110.3 . . ?
H41B C41 H41D 129.8 . . ?
H41C C41 H41D 108.6 . . ?
C43 C42 C41 110.4(5) . . ?
C43 C42 H42A 109.6 . . ?
C41 C42 H42A 109.6 . . ?
C43 C42 H42B 109.6 . . ?
C41 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
C42 C43 I 111.6(4) . . ?
C42 C43 H43A 109.3 . . ?
I C43 H43A 109.3 . . ?
C42 C43 H43B 109.3 . . ?
I C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
C43A C42A C41 127.6(12) . . ?
C43A C42A H42C 105.4 . . ?
C41 C42A H42C 105.4 . . ?
C43A C42A H42D 105.4 . . ?
C41 C42A H42D 105.4 . . ?
H42C C42A H42D 106.0 . . ?
C42A C43A I 114.4(10) . . ?
C42A C43A H43C 108.7 . . ?
I C43A H43C 108.7 . . ?
C42A C43A H43D 108.7 . . ?
I C43A H43D 108.7 . . ?
H43C C43A H43D 107.6 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.310
_refine_diff_density_min         -2.518
_refine_diff_density_rms         0.079

data_global

# Attachment '18982_web_deposit_cif_file_3_MSHill_1364469754.k12msh7.cif'


data_k12msh7
#TrackingRef '18982_web_deposit_cif_file_3_MSHill_1364469754.k12msh7.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C39 H45 Be I N2), C7 H8'
_chemical_formula_sum            'C85 H98 Be2 I2 N4'
_chemical_formula_weight         1447.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   12.28900(10)
_cell_length_b                   17.64170(10)
_cell_length_c                   35.2748(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7647.54(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    133639
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       'irregular shape'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3000
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7809
_exptl_absorpt_correction_T_max  0.8123
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;


_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '779 1.0 degree images with φ and ω scans'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            81954
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         27.37
_reflns_number_total             16704
_reflns_number_gt                12285
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
;
DENZO-SCALEPACK Z. Otwinowski and W. Minor, "
Processing of X-ray Diffraction Data Collected in Oscillation Mode ",
Methods in Enzymology, Volume 276: Macromolecular Crystallography,
part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_structure_solution    
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119
;
_computing_structure_refinement  
;
Sheldrick GM (2008) Acta Crystallogr A64:112--122 and
C. B. Hübschle, G. M. Sheldrick and B. Dittrich
ShelXle: a Qt graphical user interface for SHELXL
J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
'WinGX publication routines, Farrugia,
L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0448P)²+0.9923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.040(12)
_refine_ls_number_reflns         16704
_refine_ls_number_parameters     808
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Be1 Be 0.9081(4) 0.6554(3) 0.40917(15) 0.0259(11) Uani 1 1 d . . .
I1 I 0.86786(2) 0.775573(14) 0.430003(9) 0.03515(8) Uani 1 1 d . . .
N1 N 1.0299(2) 0.63101(16) 0.39863(9) 0.0207(7) Uani 1 1 d . . .
N2 N 0.8214(2) 0.58747(16) 0.40534(9) 0.0219(7) Uani 1 1 d . . .
C1 C 1.0463(3) 0.5620(2) 0.38253(11) 0.0236(9) Uani 1 1 d . . .
C2 C 1.1555(3) 0.53830(19) 0.36759(13) 0.0253(10) Uani 1 1 d . . .
C3 C 1.2505(3) 0.5423(2) 0.38841(13) 0.0311(10) Uani 1 1 d . . .
H3 H 1.2481 0.5616 0.4135 0.037 Uiso 1 1 calc R . .
C4 C 1.3502(3) 0.5184(2) 0.37341(14) 0.0355(11) Uani 1 1 d . . .
H4 H 1.4149 0.5217 0.3881 0.043 Uiso 1 1 calc R . .
C5 C 1.3529(3) 0.4900(2) 0.33689(13) 0.0338(11) Uani 1 1 d . . .
H5 H 1.4201 0.4736 0.3264 0.041 Uiso 1 1 calc R . .
C6 C 1.2591(3) 0.4853(2) 0.31554(14) 0.0336(11) Uani 1 1 d . . .
H6 H 1.2619 0.4660 0.2904 0.040 Uiso 1 1 calc R . .
C7 C 1.1601(3) 0.5089(2) 0.33099(13) 0.0315(10) Uani 1 1 d . . .
H7 H 1.0953 0.5049 0.3164 0.038 Uiso 1 1 calc R . .
C8 C 0.9624(3) 0.5095(2) 0.37962(13) 0.0281(10) Uani 1 1 d . . .
H8 H 0.9791 0.4623 0.3681 0.034 Uiso 1 1 calc R . .
C9 C 0.8547(3) 0.5202(2) 0.39230(11) 0.0250(9) Uani 1 1 d . . .
C10 C 0.7834(3) 0.4513(2) 0.39260(13) 0.0307(10) Uani 1 1 d . . .
C11 C 0.8247(3) 0.3849(2) 0.40753(15) 0.0410(12) Uani 1 1 d . . .
H11 H 0.8968 0.3842 0.4173 0.049 Uiso 1 1 calc R . .
C12 C 0.7623(4) 0.3190(3) 0.40849(18) 0.0591(16) Uani 1 1 d . . .
H12 H 0.7919 0.2736 0.4186 0.071 Uiso 1 1 calc R . .
C13 C 0.6571(4) 0.3199(3) 0.39467(19) 0.0654(18) Uani 1 1 d . . .
H13 H 0.6135 0.2754 0.3957 0.078 Uiso 1 1 calc R . .
C14 C 0.6161(4) 0.3854(3) 0.37950(18) 0.0656(17) Uani 1 1 d . . .
H14 H 0.5441 0.3858 0.3697 0.079 Uiso 1 1 calc R . .
C15 C 0.6774(4) 0.4507(2) 0.37826(15) 0.0464(13) Uani 1 1 d . . .
H15 H 0.6474 0.4956 0.3676 0.056 Uiso 1 1 calc R . .
C16 C 1.1216(3) 0.68186(19) 0.40466(12) 0.0233(9) Uani 1 1 d . . .
C17 C 1.1661(3) 0.7214(2) 0.37442(12) 0.0256(9) Uani 1 1 d . . .
C18 C 1.1199(3) 0.7177(2) 0.33432(12) 0.0336(10) Uani 1 1 d . . .
H18 H 1.0667 0.6748 0.3335 0.040 Uiso 1 1 calc R . .
C19 C 1.2064(4) 0.7023(3) 0.30409(14) 0.0460(13) Uani 1 1 d . . .
H19A H 1.1710 0.6946 0.2795 0.069 Uiso 1 1 calc R . .
H19B H 1.2477 0.6568 0.3109 0.069 Uiso 1 1 calc R . .
H19C H 1.2559 0.7458 0.3025 0.069 Uiso 1 1 calc R . .
C20 C 1.0569(4) 0.7909(3) 0.32531(16) 0.0591(15) Uani 1 1 d . . .
H20A H 1.0240 0.7869 0.3001 0.089 Uiso 1 1 calc R . .
H20B H 1.1070 0.8342 0.3258 0.089 Uiso 1 1 calc R . .
H20C H 0.9996 0.7984 0.3443 0.089 Uiso 1 1 calc R . .
C21 C 1.2555(3) 0.7685(2) 0.38209(14) 0.0344(11) Uani 1 1 d . . .
H21 H 1.2891 0.7953 0.3619 0.041 Uiso 1 1 calc R . .
C22 C 1.2954(3) 0.7765(3) 0.41824(14) 0.0380(11) Uani 1 1 d . . .
H22 H 1.3567 0.8082 0.4227 0.046 Uiso 1 1 calc R . .
C23 C 1.2468(3) 0.7389(2) 0.44801(14) 0.0332(11) Uani 1 1 d . . .
H23 H 1.2743 0.7452 0.4730 0.040 Uiso 1 1 calc R . .
C24 C 1.1579(3) 0.6917(2) 0.44192(12) 0.0252(9) Uani 1 1 d . . .
C25 C 1.1046(3) 0.6528(2) 0.47621(12) 0.0315(10) Uani 1 1 d . . .
H25 H 1.0361 0.6279 0.4674 0.038 Uiso 1 1 calc R . .
C26 C 1.0748(4) 0.7092(2) 0.50764(14) 0.0428(12) Uani 1 1 d . . .
H26A H 1.0334 0.6830 0.5274 0.064 Uiso 1 1 calc R . .
H26B H 1.0305 0.7502 0.4970 0.064 Uiso 1 1 calc R . .
H26C H 1.1415 0.7304 0.5186 0.064 Uiso 1 1 calc R . .
C27 C 1.1786(4) 0.5911(3) 0.49344(14) 0.0517(13) Uani 1 1 d . . .
H27A H 1.1418 0.5676 0.5151 0.078 Uiso 1 1 calc R . .
H27B H 1.2470 0.6141 0.5019 0.078 Uiso 1 1 calc R . .
H27C H 1.1940 0.5524 0.4743 0.078 Uiso 1 1 calc R . .
C28 C 0.7123(3) 0.5958(2) 0.42038(11) 0.0230(9) Uani 1 1 d . . .
C29 C 0.6873(3) 0.5631(2) 0.45543(13) 0.0303(10) Uani 1 1 d . . .
C30 C 0.7697(4) 0.5227(2) 0.47982(14) 0.0384(11) Uani 1 1 d . . .
H30 H 0.8327 0.5091 0.4632 0.046 Uiso 1 1 calc R . .
C31 C 0.8117(4) 0.5768(3) 0.51005(14) 0.0509(13) Uani 1 1 d . . .
H31A H 0.8711 0.5527 0.5241 0.076 Uiso 1 1 calc R . .
H31B H 0.7525 0.5895 0.5276 0.076 Uiso 1 1 calc R . .
H31C H 0.8384 0.6232 0.4980 0.076 Uiso 1 1 calc R . .
C32 C 0.7285(5) 0.4491(3) 0.49809(16) 0.0583(15) Uani 1 1 d . . .
H32A H 0.7901 0.4213 0.5090 0.087 Uiso 1 1 calc R . .
H32B H 0.6931 0.4176 0.4788 0.087 Uiso 1 1 calc R . .
H32C H 0.6761 0.4613 0.5181 0.087 Uiso 1 1 calc R . .
C33 C 0.5811(4) 0.5736(2) 0.46921(13) 0.0409(11) Uani 1 1 d . . .
H33 H 0.5613 0.5516 0.4928 0.049 Uiso 1 1 calc R . .
C34 C 0.5057(3) 0.6145(3) 0.44961(16) 0.0439(13) Uani 1 1 d . . .
H34 H 0.4339 0.6196 0.4593 0.053 Uiso 1 1 calc R . .
C35 C 0.5331(3) 0.6482(3) 0.41611(14) 0.0384(12) Uani 1 1 d . . .
H35 H 0.4800 0.6774 0.4031 0.046 Uiso 1 1 calc R . .
C36 C 0.6375(3) 0.6410(2) 0.40032(13) 0.0295(9) Uani 1 1 d . . .
C37 C 0.6643(3) 0.6797(2) 0.36320(14) 0.0380(11) Uani 1 1 d . . .
H37 H 0.7452 0.6858 0.3623 0.046 Uiso 1 1 calc R . .
C38 C 0.6324(5) 0.6308(3) 0.32908(15) 0.0779(19) Uani 1 1 d . . .
H38A H 0.6537 0.6565 0.3056 0.117 Uiso 1 1 calc R . .
H38B H 0.5535 0.6227 0.3291 0.117 Uiso 1 1 calc R . .
H38C H 0.6695 0.5817 0.3307 0.117 Uiso 1 1 calc R . .
C39 C 0.6158(4) 0.7585(3) 0.35972(18) 0.0713(19) Uani 1 1 d . . .
H39A H 0.6442 0.7832 0.3369 0.107 Uiso 1 1 calc R . .
H39B H 0.6356 0.7886 0.3821 0.107 Uiso 1 1 calc R . .
H39C H 0.5364 0.7547 0.3580 0.107 Uiso 1 1 calc R . .
Be2 Be 0.6410(4) 0.4060(3) 0.70142(16) 0.0284(12) Uani 1 1 d . . .
I2 I 0.59685(2) 0.400465(17) 0.764346(9) 0.03996(9) Uani 1 1 d . . .
N3 N 0.7616(2) 0.41976(17) 0.68466(10) 0.0237(8) Uani 1 1 d . . .
N4 N 0.5508(2) 0.40210(18) 0.66788(10) 0.0257(8) Uani 1 1 d . . .
C40 C 0.7733(3) 0.4412(2) 0.64801(13) 0.0238(9) Uani 1 1 d . . .
C41 C 0.8806(3) 0.4582(2) 0.63047(11) 0.0272(9) Uani 1 1 d . . .
C42 C 0.9639(3) 0.4050(3) 0.62855(15) 0.0524(14) Uani 1 1 d . . .
H42 H 0.9548 0.3573 0.6406 0.063 Uiso 1 1 calc R . .
C43 C 1.0593(4) 0.4200(4) 0.60961(18) 0.073(2) Uani 1 1 d . . .
H43 H 1.1143 0.3824 0.6081 0.088 Uiso 1 1 calc R . .
C44 C 1.0750(3) 0.4901(3) 0.59279(15) 0.0548(15) Uani 1 1 d . . .
H44 H 1.1408 0.5007 0.5797 0.066 Uiso 1 1 calc R . .
C45 C 0.9956(4) 0.5438(3) 0.59517(14) 0.0456(13) Uani 1 1 d . . .
H45 H 1.0070 0.5923 0.5842 0.055 Uiso 1 1 calc R . .
C46 C 0.8973(3) 0.5281(2) 0.61366(12) 0.0338(10) Uani 1 1 d . . .
H46 H 0.8419 0.5656 0.6147 0.041 Uiso 1 1 calc R . .
C47 C 0.6832(3) 0.4466(2) 0.62375(12) 0.0248(9) Uani 1 1 d . . .
H47 H 0.6959 0.4660 0.5990 0.030 Uiso 1 1 calc R . .
C48 C 0.5753(3) 0.42605(19) 0.63280(12) 0.0223(9) Uani 1 1 d . . .
C49 C 0.4953(3) 0.4329(2) 0.60170(13) 0.0277(10) Uani 1 1 d . . .
C50 C 0.4888(3) 0.5017(2) 0.58166(12) 0.0299(10) Uani 1 1 d . . .
H50 H 0.5345 0.5428 0.5887 0.036 Uiso 1 1 calc R . .
C51 C 0.4166(3) 0.5103(2) 0.55179(13) 0.0346(10) Uani 1 1 d . . .
H51 H 0.4120 0.5578 0.5391 0.042 Uiso 1 1 calc R . .
C52 C 0.3515(4) 0.4514(2) 0.54021(14) 0.0434(12) Uani 1 1 d . . .
H52 H 0.3028 0.4575 0.5195 0.052 Uiso 1 1 calc R . .
C53 C 0.3584(4) 0.3823(3) 0.55959(16) 0.0584(16) Uani 1 1 d . . .
H53 H 0.3150 0.3407 0.5517 0.070 Uiso 1 1 calc R . .
C54 C 0.4275(4) 0.3743(2) 0.58994(16) 0.0495(14) Uani 1 1 d . . .
H54 H 0.4289 0.3276 0.6033 0.059 Uiso 1 1 calc R . .
C55 C 0.8583(3) 0.4132(2) 0.70832(11) 0.0246(9) Uani 1 1 d . . .
C56 C 0.8965(3) 0.3407(2) 0.71730(12) 0.0283(10) Uani 1 1 d . . .
C57 C 0.8426(3) 0.2689(2) 0.70370(13) 0.0347(10) Uani 1 1 d . . .
H57 H 0.7826 0.2835 0.6860 0.042 Uiso 1 1 calc R . .
C58 C 0.7915(3) 0.2244(3) 0.73698(15) 0.0440(12) Uani 1 1 d . . .
H58A H 0.7506 0.1811 0.7271 0.066 Uiso 1 1 calc R . .
H58B H 0.7423 0.2578 0.7511 0.066 Uiso 1 1 calc R . .
H58C H 0.8492 0.2063 0.7539 0.066 Uiso 1 1 calc R . .
C59 C 0.9208(4) 0.2160(3) 0.68190(15) 0.0519(13) Uani 1 1 d . . .
H59A H 0.8785 0.1790 0.6673 0.078 Uiso 1 1 calc R . .
H59B H 0.9678 0.1893 0.7000 0.078 Uiso 1 1 calc R . .
H59C H 0.9658 0.2461 0.6646 0.078 Uiso 1 1 calc R . .
C60 C 0.9891(3) 0.3351(2) 0.74008(13) 0.0342(11) Uani 1 1 d . . .
H60 H 1.0164 0.2865 0.7466 0.041 Uiso 1 1 calc R . .
C61 C 1.0417(3) 0.3994(3) 0.75328(12) 0.0372(11) Uani 1 1 d . . .
H61 H 1.1061 0.3946 0.7680 0.045 Uiso 1 1 calc R . .
C62 C 1.0008(3) 0.4700(3) 0.74514(12) 0.0334(11) Uani 1 1 d . . .
H62 H 1.0363 0.5136 0.7550 0.040 Uiso 1 1 calc R . .
C63 C 0.9084(3) 0.4789(2) 0.72274(12) 0.0296(10) Uani 1 1 d . . .
C64 C 0.8642(3) 0.5584(2) 0.71653(13) 0.0327(10) Uani 1 1 d . . .
H64 H 0.8074 0.5552 0.6963 0.039 Uiso 1 1 calc R . .
C65 C 0.8086(4) 0.5878(3) 0.75257(14) 0.0492(13) Uani 1 1 d . . .
H65A H 0.7818 0.6394 0.7482 0.074 Uiso 1 1 calc R . .
H65B H 0.8611 0.5883 0.7735 0.074 Uiso 1 1 calc R . .
H65C H 0.7474 0.5547 0.7591 0.074 Uiso 1 1 calc R . .
C66 C 0.9509(4) 0.6133(2) 0.70290(15) 0.0438(13) Uani 1 1 d . . .
H66A H 0.9176 0.6627 0.6977 0.066 Uiso 1 1 calc R . .
H66B H 0.9843 0.5937 0.6797 0.066 Uiso 1 1 calc R . .
H66C H 1.0068 0.6190 0.7225 0.066 Uiso 1 1 calc R . .
C67 C 0.4401(3) 0.3770(2) 0.67573(12) 0.0277(10) Uani 1 1 d . . .
C68 C 0.3554(3) 0.4296(2) 0.67814(13) 0.0331(10) Uani 1 1 d . . .
C69 C 0.3737(3) 0.5148(2) 0.67733(13) 0.0328(10) Uani 1 1 d . . .
H69 H 0.4501 0.5246 0.6688 0.039 Uiso 1 1 calc R . .
C70 C 0.3600(4) 0.5473(3) 0.71647(15) 0.0540(14) Uani 1 1 d . . .
H70A H 0.3696 0.6024 0.7155 0.081 Uiso 1 1 calc R . .
H70B H 0.4146 0.5252 0.7335 0.081 Uiso 1 1 calc R . .
H70C H 0.2870 0.5354 0.7259 0.081 Uiso 1 1 calc R . .
C71 C 0.2969(3) 0.5560(3) 0.65067(15) 0.0448(13) Uani 1 1 d . . .
H71A H 0.3135 0.6103 0.6509 0.067 Uiso 1 1 calc R . .
H71B H 0.2217 0.5481 0.6590 0.067 Uiso 1 1 calc R . .
H71C H 0.3060 0.5362 0.6249 0.067 Uiso 1 1 calc R . .
C72 C 0.2517(3) 0.4011(3) 0.68314(15) 0.0456(13) Uani 1 1 d . . .
H72 H 0.1924 0.4355 0.6849 0.055 Uiso 1 1 calc R . .
C73 C 0.2314(3) 0.3244(3) 0.68560(16) 0.0494(14) Uani 1 1 d . . .
H73 H 0.1586 0.3065 0.6874 0.059 Uiso 1 1 calc R . .
C74 C 0.3172(3) 0.2733(3) 0.68546(14) 0.0399(12) Uani 1 1 d . . .
H74 H 0.3033 0.2207 0.6885 0.048 Uiso 1 1 calc R . .
C75 C 0.4247(3) 0.2991(2) 0.68080(13) 0.0297(10) Uani 1 1 d . . .
C76 C 0.5188(3) 0.2431(2) 0.68286(13) 0.0338(11) Uani 1 1 d . . .
H76 H 0.5785 0.2688 0.6972 0.041 Uiso 1 1 calc R . .
C77 C 0.4919(4) 0.1703(2) 0.70447(16) 0.0525(14) Uani 1 1 d . . .
H77A H 0.5593 0.1428 0.7100 0.079 Uiso 1 1 calc R . .
H77B H 0.4441 0.1384 0.6890 0.079 Uiso 1 1 calc R . .
H77C H 0.4550 0.1831 0.7283 0.079 Uiso 1 1 calc R . .
C78 C 0.5651(4) 0.2226(3) 0.64393(14) 0.0458(12) Uani 1 1 d . . .
H78A H 0.6275 0.1886 0.6471 0.069 Uiso 1 1 calc R . .
H78B H 0.5886 0.2689 0.6309 0.069 Uiso 1 1 calc R . .
H78C H 0.5090 0.1972 0.6288 0.069 Uiso 1 1 calc R . .
C81 C 0.2043(6) 0.3094(5) 0.4476(2) 0.153(4) Uiso 1 1 d G . .
C82 C 0.1558(6) 0.3797(4) 0.4534(2) 0.144(3) Uiso 1 1 d G . .
H82 H 0.1809 0.4227 0.4398 0.173 Uiso 1 1 calc R . .
C83 C 0.0706(6) 0.3869(4) 0.4790(2) 0.142(3) Uiso 1 1 d G . .
H83 H 0.0374 0.4349 0.4830 0.170 Uiso 1 1 calc R . .
C84 C 0.0339(6) 0.3239(6) 0.4989(2) 0.239(7) Uiso 1 1 d G . .
H84 H -0.0244 0.3289 0.5165 0.287 Uiso 1 1 calc R . .
C85 C 0.0823(9) 0.2537(4) 0.4932(3) 0.249(7) Uiso 1 1 d G . .
H85 H 0.0572 0.2106 0.5068 0.298 Uiso 1 1 calc R . .
C86 C 0.1675(8) 0.2464(4) 0.4675(3) 0.244(7) Uiso 1 1 d G . .
H86 H 0.2007 0.1984 0.4636 0.292 Uiso 1 1 calc R . .
C87 C 0.3101(12) 0.3056(8) 0.4259(4) 0.233(6) Uiso 1 1 d . . .
H87A H 0.3281 0.2526 0.4206 0.350 Uiso 1 1 calc R . .
H87B H 0.3684 0.3285 0.4411 0.350 Uiso 1 1 calc R . .
H87C H 0.3026 0.3334 0.4020 0.350 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Be1 N1 1.602(6) . ?
Be1 N2 1.608(6) . ?
Be1 I1 2.298(5) . ?
N1 C1 1.359(5) . ?
N1 C16 1.456(4) . ?
N2 C9 1.337(4) . ?
N2 C28 1.450(4) . ?
C1 C8 1.390(5) . ?
C1 C2 1.501(5) . ?
C2 C3 1.381(6) . ?
C2 C7 1.393(6) . ?
C3 C4 1.399(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.410(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.497(5) . ?
C10 C11 1.381(6) . ?
C10 C15 1.398(6) . ?
C11 C12 1.394(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.370(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.387(5) . ?
C16 C24 1.399(5) . ?
C17 C21 1.404(5) . ?
C17 C18 1.526(6) . ?
C18 C19 1.530(6) . ?
C18 C20 1.540(6) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.374(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.537(6) . ?
C25 C26 1.534(6) . ?
C25 C27 1.542(6) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.399(6) . ?
C28 C36 1.407(5) . ?
C29 C33 1.404(6) . ?
C29 C30 1.508(6) . ?
C30 C31 1.522(6) . ?
C30 C32 1.535(6) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.364(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.365(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.405(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.513(6) . ?
C37 C39 1.517(6) . ?
C37 C38 1.533(7) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
Be2 N3 1.614(6) . ?
Be2 N4 1.623(6) . ?
Be2 I2 2.287(6) . ?
N3 C40 1.354(5) . ?
N3 C55 1.457(5) . ?
N4 C48 1.342(5) . ?
N4 C67 1.457(5) . ?
C40 C47 1.403(5) . ?
C40 C41 1.488(5) . ?
C41 C46 1.384(5) . ?
C41 C42 1.390(6) . ?
C42 C43 1.374(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.362(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.400(6) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.411(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.478(6) . ?
C49 C54 1.391(6) . ?
C49 C50 1.408(6) . ?
C50 C51 1.386(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.373(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.401(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.374(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.399(5) . ?
C55 C63 1.408(5) . ?
C56 C60 1.397(6) . ?
C56 C57 1.507(6) . ?
C57 C59 1.545(6) . ?
C57 C58 1.545(6) . ?
C57 H57 1.0000 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.386(6) . ?
C60 H60 0.9500 . ?
C61 C62 1.374(6) . ?
C61 H61 0.9500 . ?
C62 C63 1.392(6) . ?
C62 H62 0.9500 . ?
C63 C64 1.520(5) . ?
C64 C66 1.518(6) . ?
C64 C65 1.534(6) . ?
C64 H64 1.0000 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C68 1.397(5) . ?
C67 C75 1.398(5) . ?
C68 C72 1.382(5) . ?
C68 C69 1.521(5) . ?
C69 C70 1.504(6) . ?
C69 C71 1.518(6) . ?
C69 H69 1.0000 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.378(6) . ?
C72 H72 0.9500 . ?
C73 C74 1.387(6) . ?
C73 H73 0.9500 . ?
C74 C75 1.407(5) . ?
C74 H74 0.9500 . ?
C75 C76 1.523(5) . ?
C76 C77 1.529(6) . ?
C76 C78 1.530(6) . ?
C76 H76 1.0000 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C81 C82 1.3900 . ?
C81 C86 1.3900 . ?
C81 C87 1.511(14) . ?
C82 C83 1.3900 . ?
C82 H82 0.9500 . ?
C83 C84 1.3900 . ?
C83 H83 0.9500 . ?
C84 C85 1.3900 . ?
C84 H84 0.9500 . ?
C85 C86 1.3900 . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Be1 N2 113.5(3) . . ?
N1 Be1 I1 121.5(3) . . ?
N2 Be1 I1 124.9(3) . . ?
C1 N1 C16 119.9(3) . . ?
C1 N1 Be1 118.5(3) . . ?
C16 N1 Be1 121.6(3) . . ?
C9 N2 C28 119.9(3) . . ?
C9 N2 Be1 119.2(3) . . ?
C28 N2 Be1 120.4(3) . . ?
N1 C1 C8 121.2(3) . . ?
N1 C1 C2 121.9(3) . . ?
C8 C1 C2 116.9(3) . . ?
C3 C2 C7 118.5(4) . . ?
C3 C2 C1 123.7(4) . . ?
C7 C2 C1 117.7(3) . . ?
C2 C3 C4 121.6(4) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C6 120.5(4) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C1 C8 C9 125.8(4) . . ?
C1 C8 H8 117.1 . . ?
C9 C8 H8 117.1 . . ?
N2 C9 C8 120.9(3) . . ?
N2 C9 C10 122.6(3) . . ?
C8 C9 C10 116.3(3) . . ?
C11 C10 C15 118.3(4) . . ?
C11 C10 C9 118.4(4) . . ?
C15 C10 C9 123.3(4) . . ?
C10 C11 C12 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 119.8(5) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 119.5(5) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 121.2(5) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C14 C15 C10 120.3(5) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C17 C16 C24 122.3(3) . . ?
C17 C16 N1 120.2(4) . . ?
C24 C16 N1 117.4(3) . . ?
C16 C17 C21 117.3(4) . . ?
C16 C17 C18 123.0(3) . . ?
C21 C17 C18 119.7(4) . . ?
C17 C18 C19 113.3(4) . . ?
C17 C18 C20 110.1(4) . . ?
C19 C18 C20 110.7(4) . . ?
C17 C18 H18 107.5 . . ?
C19 C18 H18 107.5 . . ?
C20 C18 H18 107.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C17 121.3(4) . . ?
C22 C21 H21 119.3 . . ?
C17 C21 H21 119.3 . . ?
C21 C22 C23 120.1(4) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C24 120.8(4) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C16 118.0(4) . . ?
C23 C24 C25 118.7(4) . . ?
C16 C24 C25 123.2(3) . . ?
C26 C25 C24 112.4(3) . . ?
C26 C25 C27 108.3(4) . . ?
C24 C25 C27 112.0(3) . . ?
C26 C25 H25 108.0 . . ?
C24 C25 H25 108.0 . . ?
C27 C25 H25 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C36 122.3(3) . . ?
C29 C28 N2 119.0(3) . . ?
C36 C28 N2 118.5(3) . . ?
C28 C29 C33 117.1(4) . . ?
C28 C29 C30 123.5(4) . . ?
C33 C29 C30 119.3(4) . . ?
C29 C30 C31 109.3(4) . . ?
C29 C30 C32 114.7(4) . . ?
C31 C30 C32 110.4(4) . . ?
C29 C30 H30 107.4 . . ?
C31 C30 H30 107.4 . . ?
C32 C30 H30 107.4 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C29 121.7(5) . . ?
C34 C33 H33 119.1 . . ?
C29 C33 H33 119.1 . . ?
C33 C34 C35 120.1(4) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 122.0(4) . . ?
C34 C35 H35 119.0 . . ?
C36 C35 H35 119.0 . . ?
C35 C36 C28 116.6(4) . . ?
C35 C36 C37 120.1(4) . . ?
C28 C36 C37 123.3(4) . . ?
C36 C37 C39 113.5(4) . . ?
C36 C37 C38 111.7(4) . . ?
C39 C37 C38 110.6(4) . . ?
C36 C37 H37 106.9 . . ?
C39 C37 H37 106.9 . . ?
C38 C37 H37 106.9 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N3 Be2 N4 111.5(4) . . ?
N3 Be2 I2 125.4(3) . . ?
N4 Be2 I2 122.9(3) . . ?
C40 N3 C55 118.8(3) . . ?
C40 N3 Be2 119.3(3) . . ?
C55 N3 Be2 121.8(3) . . ?
C48 N4 C67 118.8(3) . . ?
C48 N4 Be2 120.3(3) . . ?
C67 N4 Be2 120.8(3) . . ?
N3 C40 C47 121.2(3) . . ?
N3 C40 C41 123.2(3) . . ?
C47 C40 C41 115.6(4) . . ?
C46 C41 C42 118.1(4) . . ?
C46 C41 C40 119.3(3) . . ?
C42 C41 C40 122.5(4) . . ?
C43 C42 C41 121.4(5) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C42 C43 C44 120.0(5) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C45 C44 C43 119.6(4) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C46 120.6(4) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C41 C46 C45 120.2(4) . . ?
C41 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C40 C47 C48 125.9(4) . . ?
C40 C47 H47 117.1 . . ?
C48 C47 H47 117.1 . . ?
N4 C48 C47 120.1(3) . . ?
N4 C48 C49 124.1(3) . . ?
C47 C48 C49 115.8(4) . . ?
C54 C49 C50 117.2(4) . . ?
C54 C49 C48 124.0(4) . . ?
C50 C49 C48 118.8(3) . . ?
C51 C50 C49 120.9(4) . . ?
C51 C50 H50 119.6 . . ?
C49 C50 H50 119.6 . . ?
C52 C51 C50 121.1(4) . . ?
C52 C51 H51 119.5 . . ?
C50 C51 H51 119.5 . . ?
C51 C52 C53 118.6(4) . . ?
C51 C52 H52 120.7 . . ?
C53 C52 H52 120.7 . . ?
C54 C53 C52 120.5(4) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C49 121.8(4) . . ?
C53 C54 H54 119.1 . . ?
C49 C54 H54 119.1 . . ?
C56 C55 C63 121.6(3) . . ?
C56 C55 N3 118.5(3) . . ?
C63 C55 N3 119.9(3) . . ?
C60 C56 C55 117.9(4) . . ?
C60 C56 C57 118.8(3) . . ?
C55 C56 C57 123.3(4) . . ?
C56 C57 C59 113.1(3) . . ?
C56 C57 C58 111.3(4) . . ?
C59 C57 C58 108.9(4) . . ?
C56 C57 H57 107.8 . . ?
C59 C57 H57 107.8 . . ?
C58 C57 H57 107.8 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 C56 121.0(4) . . ?
C61 C60 H60 119.5 . . ?
C56 C60 H60 119.5 . . ?
C62 C61 C60 120.1(4) . . ?
C62 C61 H61 120.0 . . ?
C60 C61 H61 120.0 . . ?
C61 C62 C63 121.3(4) . . ?
C61 C62 H62 119.4 . . ?
C63 C62 H62 119.4 . . ?
C62 C63 C55 118.0(4) . . ?
C62 C63 C64 118.5(4) . . ?
C55 C63 C64 123.4(3) . . ?
C66 C64 C63 112.5(4) . . ?
C66 C64 C65 111.1(4) . . ?
C63 C64 C65 110.6(4) . . ?
C66 C64 H64 107.5 . . ?
C63 C64 H64 107.5 . . ?
C65 C64 H64 107.5 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 C75 122.9(3) . . ?
C68 C67 N4 120.3(3) . . ?
C75 C67 N4 116.8(3) . . ?
C72 C68 C67 117.0(4) . . ?
C72 C68 C69 119.9(4) . . ?
C67 C68 C69 123.1(3) . . ?
C70 C69 C71 108.5(4) . . ?
C70 C69 C68 110.0(4) . . ?
C71 C69 C68 113.1(4) . . ?
C70 C69 H69 108.4 . . ?
C71 C69 H69 108.4 . . ?
C68 C69 H69 108.4 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C73 C72 C68 122.1(4) . . ?
C73 C72 H72 118.9 . . ?
C68 C72 H72 118.9 . . ?
C72 C73 C74 120.0(4) . . ?
C72 C73 H73 120.0 . . ?
C74 C73 H73 120.0 . . ?
C73 C74 C75 120.2(4) . . ?
C73 C74 H74 119.9 . . ?
C75 C74 H74 119.9 . . ?
C67 C75 C74 117.4(4) . . ?
C67 C75 C76 122.7(3) . . ?
C74 C75 C76 119.9(3) . . ?
C75 C76 C77 113.8(4) . . ?
C75 C76 C78 113.1(4) . . ?
C77 C76 C78 109.2(4) . . ?
C75 C76 H76 106.7 . . ?
C77 C76 H76 106.7 . . ?
C78 C76 H76 106.7 . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C76 C78 H78A 109.5 . . ?
C76 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C76 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C82 C81 C86 120.0 . . ?
C82 C81 C87 118.9(8) . . ?
C86 C81 C87 120.0(8) . . ?
C81 C82 C83 120.0 . . ?
C81 C82 H82 120.0 . . ?
C83 C82 H82 120.0 . . ?
C84 C83 C82 120.0 . . ?
C84 C83 H83 120.0 . . ?
C82 C83 H83 120.0 . . ?
C83 C84 C85 120.0 . . ?
C83 C84 H84 120.0 . . ?
C85 C84 H84 120.0 . . ?
C84 C85 C86 120.0 . . ?
C84 C85 H85 120.0 . . ?
C86 C85 H85 120.0 . . ?
C85 C86 C81 120.0 . . ?
C85 C86 H86 120.0 . . ?
C81 C86 H86 120.0 . . ?
C81 C87 H87A 109.5 . . ?
C81 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C81 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        27.37
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.079


